WO2003086566A2 - Procede et dispositif permettant d'extraire des substances de vegetaux - Google Patents

Procede et dispositif permettant d'extraire des substances de vegetaux Download PDF

Info

Publication number
WO2003086566A2
WO2003086566A2 PCT/EP2003/004150 EP0304150W WO03086566A2 WO 2003086566 A2 WO2003086566 A2 WO 2003086566A2 EP 0304150 W EP0304150 W EP 0304150W WO 03086566 A2 WO03086566 A2 WO 03086566A2
Authority
WO
WIPO (PCT)
Prior art keywords
plants
plant
container
fluid medium
parts
Prior art date
Application number
PCT/EP2003/004150
Other languages
German (de)
English (en)
Other versions
WO2003086566A3 (fr
Inventor
Elke Foltys De Garcia
Emmerich Tetkov
Original Assignee
Elke Foltys De Garcia
Emmerich Tetkov
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Elke Foltys De Garcia, Emmerich Tetkov filed Critical Elke Foltys De Garcia
Priority to AU2003233038A priority Critical patent/AU2003233038A1/en
Publication of WO2003086566A2 publication Critical patent/WO2003086566A2/fr
Publication of WO2003086566A3 publication Critical patent/WO2003086566A3/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0219—Fixed bed of solid material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • B01D11/0284—Multistage extraction

Definitions

  • the present invention relates to a method and an apparatus for obtaining plant ingredients.
  • the invention relates to a method and an apparatus with which plant ingredients can be distilled by steam and / or extracted using any solvent.
  • the invention relates to a method and a device for obtaining plant ingredients in essentially free form from decomposition products, secondary products and / or undesired components by means of steam distillation and / or solvent extraction.
  • a further disadvantage was that in cases in which a successive treatment of plants or parts of plants with water and solvent was desired, components which were successively water-soluble or miscible with water on the one hand and components which were not water-soluble or miscible with water on the other to win, the plants or their parts removed from the device for the steam treatment and into another device for the non-aqueous Treatment had to be filled, since it is known that the device used for the treatment with water (steam) is not suitable for treating the plants or parts of plants with solvent (s).
  • the object of the invention was therefore to provide a method and a device with which the extraction of plant constituents can be carried out successively, but without changing the device, both by steam distillation and by solvent extraction.
  • the method and device should be designed in such a way that existing systems can preferably be retrofitted in such a way that the retrofitted parts enable both procedures and existing parts can largely be used.
  • the invention therefore relates to a method for obtaining one or more plant ingredients ⁇ ) from plants and / or parts of plants according to claim 1. Preferred embodiments of the method are claimed in dependent claims 2 to 16. The invention also relates to a device for obtaining one or more plant constituents (s) from plants and / or parts of plants according to claim 17. Preferred embodiments of the devices are claimed in claims 18 to 23.
  • the invention also relates to the use of the device for obtaining one or more plant ingredients according to claim 24.
  • plant ingredients are obtained from plants and or parts of plants.
  • plant constituents are understood to mean those chemical substances which are contained in plants and / or parts of plants and which are intended to be obtained for the purposes of further use or further processing.
  • special embodiments of plant constituents are aroma substances (flavorings), fragrances, seasonings, plant colorants, plant active substances, plant poisons, drugs or the like.
  • a single plant and / or plant parts can be contained therein within the scope of the present process
  • Plant ingredient can be obtained, or several ingredients can be obtained.
  • plants are plants which contain at least one ingredient, the extraction of which is of interest for further use or further processing.
  • Plant parts can be any parts of plants and, in the context of the present invention, are preferably leaves, stems, roots, buds, flowers, fruits, seeds and shoots of plants falling under the above definition or mixtures of one or more of the aforementioned plant parts.
  • the process steps can be an isolated steam distillation or an isolated solvent extraction carried out instead.
  • the process steps can however, in a process consisting of two steps, solvent extraction in an earlier process step and steam distillation in a later process step or steam distillation in an earlier process step and solvent extraction in a later process step.
  • the sequence of steam distillation in the earlier step and solvent distillation in a subsequent later step is the most preferred procedure according to the invention. Based on this, the invention will be explained in more detail later, without being limited to this sequence of steps.
  • Figure 1 is a schematic of the method based on the essential parts of the device according to the invention.
  • Figure 2 A is a plan view of a combined steam distillation and solvent extraction plant according to the invention with separate top covers and bottom attachments of the cylindrical container;
  • FIG. 2B shows a detailed side sectional view of the installation according to FIG. 2A;
  • FIG. 3A shows a top view of a combined steam distillation and solvent extraction installation according to the invention with a single upper cover and a single lower attachment of the cylindrical container;
  • Figure 3 B is a detailed side sectional view of the system of Figure 3 A;
  • Figure 4 is a sectional view of an upper cover of the cylindrical container for steam distillation; and Figure 5 is a sectional view of an upper cover of the cylindrical solvent extraction container.
  • the inventive method for obtaining one or more plant ingredients ⁇ ) from plants and / or plant parts by treating the plants and / or plant parts with at least one fluid medium under conditions of pressure and temperature at which the plants and / or plant parts one or Dispensing at least partially several plant constituent (s) to the at least one fluid medium, and separating the plant constituent (s) from the at least one fluid medium comprises the steps that a preferably cylindrical container with one in one preferred embodiment, the quantity of plants and / or plant parts measured beforehand is filled to such a density that fluid contact of the plants and / or plant parts with at least one fluid medium is possible; at least one fluid medium is fed to the cylindrical container under conditions in which an exchange of one or more plant constituent (s) between the plants and / or plant parts on the one hand and the fluid medium on the other hand is possible; the fluid medium comprising at least one, one or more plant constituent (s) from the cylindrical container supplies at least one device for separating the plant constituent (s) from the at least one fluid medium and a separation into the at least one fluid medium and perform
  • plant ingredients are obtained from plants and / or plant parts of any condition.
  • live plants and / or come Plant parts into question if the plant ingredients can best or preferably be obtained from them; freshly harvested plants or parts of plants or already withered plants or parts of plants are particularly preferred according to the invention.
  • fresh and withered plants or parts of plants side by side if this is required in practice or if this is sensible and leads to success in individual cases.
  • Dried plants or their parts e.g. roots or fruits of plants
  • whole plants or individual parts thereof such as leaves, fruits, stems, seeds, flowers, buds, roots can be used. It is also possible to use whole plants in addition to parts of plants.
  • whole plants or large plant parts are used for the process according to the invention, these can be used without comminution if the size allows filling into the cylindrical container for distillation or extraction. If the plants or parts of plants are of a size which does not permit filling into the cylindrical container, the plants and / or parts of plants are comminuted in the usual way. The degree of shredding can be chosen as desired. In preferred embodiments of the method, comminution is carried out in such a way that the parts of the plants or the plants are comminuted as little as possible in order to prevent the plant constituents contained in the plants or plant parts from interacting with air (risk of constituents being damaged by oxygen).
  • Non-limiting examples of fluid media include compounds from the group consisting of water, steam or mixtures thereof, organic solvents such as alcohols (for example methanol, ethanol, n-propanol, i-propanol, n- Butanol, sec-butanol, tert-butanol, n-pentanol and its isomers, n-hexanol and its isomers etc.) and mixtures of alcohols, polyhydric alcohols (such as ethylene glycol, propylene glycol, butylene glycol etc., glycerol or polyols such as oligomers of the Ethylene oxide), ethers (such as dimethyl ether, methyl ethyl ether, diethyl ether, methyl n-propyl ether, ethyl n-propyl ether, di-n-propyl ether, higher eth it including cyclic ethers such as tetrahydrofuran etc
  • plants or parts of plants are treated with at least one fluid medium; this also includes treatment with several fluid media.
  • the treatment with a plurality of fluid media for example with two fluid media or with three fluid media, can be carried out simultaneously by two or more than two fluid media acting simultaneously on all plants or parts of plants, or can be carried out in successive treatment steps by two or more than two fluid media are brought into contact with all plants or parts of plants in succession.
  • the plants or parts of plants are treated with one or more fluid medium / media under conditions of pressure and temperature at which the plants or parts of plants apply one or more plant constituent (s) to the at least one fluid medium, at least in part submit.
  • the temperature and pressure conditions that are used in detail depend strongly on the respective plant or the respective plant parts, on the (at least one) fluid medium used, on the possible duration of treatment and possibly also on the plant ingredient to be obtained ( as well as possibly from further parameters).
  • the treatment with water / steam is usually carried out at a pressure in the narrow range around atmospheric pressure, e.g. B. at 1.013 bar ⁇ 0.1 bar performed; however, values of pressure above or below, including vacuum, are applicable.
  • the plant ingredient (s) which at least partially were obtained from the plants or parts of plants by the procedure described above are / are separated from the at least one fluid medium.
  • This can be done by anyone in the booth Technically conceivable or also special, new processes take place as long as a clean and essentially no traces of impurities and / or traces of the fluid medium / the fluid media fraction of the plant constituent (s) obtained are obtained by this process step.
  • a cylindrical container is preferably used for the actual process of treating the plants or parts of plants. Basically, vessels of other shapes, as are known to those skilled in the art, can of course be used; However, cylindrical containers have proven themselves in practice and can therefore be used with particular advantage.
  • the cylindrical container can be made of any material that does not interact with the plants or parts of plants to be treated. Cylindrical containers made of glass, ceramic (s) or of (on the treatment side), for example, materials coated with glass, plastic or the like, such as ceramics, metals or plastics, as well as cylindrical vessels made of corrosion-free metals or precious metals or alloys of metals have proven particularly useful cylindrical vessels made of glass or one or more metal / metal alloys are particularly preferred.
  • the cylindrical container is protected against heat loss by suitable insulation and, moreover, is designed in such a way that it is also possible to apply excess pressure and / or to apply a vacuum without this leading to problems with the stability.
  • the cylindrical container can have any size suitable for the required throughput quantities of plants or parts of plants.
  • Suitable sizes are, for example - without restricting the invention by this information - on a semi-industrial scale in the range from 300 mm to 2,000 mm, preferably from 1,000 mm to 1,800 mm in height and in the range from 20 mm to 150 mm, preferably from 60 mm to 125 mm in diameter and for example on an industrial scale in the range from 1,500 mm to 5,000 mm, preferably from 1,700 mm to 5,000 mm in height and in the range from 150 mm to 1,000 mm, preferably from 250 mm to 1,000 mm in diameter , Particularly preferred and therefore advantageously usable dimensions for the technical field are in the range from 2,000 mm to 4,000 mm in height and in the range from 500 mm to 800 mm in diameter.
  • cylindrical containers are preferably used according to the invention, which are closed except for the feed lines or discharge lines. This is explained in detail below in connection with the description of the device according to the invention.
  • a closed container means that the head and the base of the container have devices which effect a closure, for example lids or covers or devices which allow air to enter or liquids to escape prevent from the cylindrical container.
  • a previously measured amount of plants and / or plant parts is filled into the cylindrical container for treating the plants or plant parts with a fluid.
  • the amount of plants or parts of plants or mixtures thereof to be filled in depends on the type of plants or parts of plants, on the respective plant (part) type, on the type of treatment, on the duration of treatment, on the treatment temperature and, if appropriate, other parameters such as, for example The degree of freshness and / or the degree of comminution of the plants (parts) and can be determined by a person skilled in the art in a few preliminary tests. For example, when using whole plants, lower filling densities will have to be selected than when using leaves or fruits. Furthermore, peppermint leaves, for example, are packed in a smaller amount in the fresh state than those in the withered state.
  • peppercorns are packed more densely than rosemary in the form of a stem or needle.
  • the pack of the plants (parts) during treatment by steam distillation can be the same as in treatment by solvent extraction. Plants (parts) that release one or more plant constituents contained therein only after swelling with a solvent may only be packed at a lower fill level than those in which the release of plant constituent (s) is therefore without swelling takes place because these are contained in near-surface plant compartments; etc. etc.
  • the amount of plants or their parts is adjusted so that the total volume of the cylindrical container for the. Treatment is available and contact with the fluid or fluids is possible for all plants or parts of plants in the cylindrical vessel.
  • the filling step takes place regularly (though not exclusively) from the top of the cylindrical vessel; the plants or parts of plants fall or sink onto a device such as a sieve or perforated plate with openings which are preferably uniformly distributed over the entire surface and which allow the fluid (s) to pass easily in both directions, but the plants or their parts Not. As a result, the fluid or the fluids later flow uniformly to the phase consisting of plants or their parts.
  • the cylindrical container is then closed again.
  • the predetermined amount of plants or parts of plants is poured into the cylindrical container in a uniformly dense bed.
  • the cylindrical containers with the therein positioned ⁇ coated plants or parts thereof is supplied to at least one fluid medium.
  • the at least one fluid medium can be one or more of the fluids mentioned above in detail.
  • the preferred direction of Zu decisions in preferred Ver ⁇ drive have to be so the invention is that a fluid or more fluids to the Ex Thermali- ons container and thus the layer of plants or plant parts is / are fed from below, that is from the foot of the cylindrical container. This is the case, for example, with steam distillation.
  • water and / or water vapor which was generated, for example, by means of a conventional steam generator, is fed to the cylindrical container at the foot thereof, either directly or via a steam relaxation space, in which the water vapor is placed under a device provided with holes or openings, such as a sieve plate distributed and then passed through this and brought into contact with the plant material or plant parts in ascending direction above the sieve tray.
  • a device provided with holes or openings such as a sieve plate distributed and then passed through this and brought into contact with the plant material or plant parts in ascending direction above the sieve tray.
  • the preferred direction of supplying at least one fluid can alternatively be such that one or more fluids are / are fed to the cylindrical vessel and thus the layer of plants or plant parts from above, that is to say from the head of the cylindrical container. This is the case, for example, with solvent extraction.
  • a fluid or several fluids are fed from the container head in a downward flowing direction to the cylindrical container and thus to the plants or parts of plants, until the inner volume of the container - apart from the plants or parts of plants - with the / the fluid (s) is flooded.
  • the fluid (s) charged with the plant constituent (s) will become downward from the cylindrical vessel drained and replaced with new fluid (s) from above. This can be done continuously or batchwise.
  • the contact between the at least one fluid and the plants or parts of plants takes place under conditions in which an exchange of one or more plant constituents) is possible between the plants and / or parts of plants.
  • These conditions for example the flow rate of the fluid (s), temperature, pressure
  • these conditions are largely dependent on the current conditions of the individual case, such as e.g. B. the type of plant, the degree of comminution of the plants or plant parts used, the height of the cylindrical container, the fluid medium used or the fluid media used, the nature of the plant constituents to be extracted) or the location in the plants or plant parts at which the plant constituent (s) is / are naturally arranged.
  • the temperature is usually at least slightly elevated and is between 70 and 140 ° C., preferably at 90 to 110 ° C. or slightly above, in the case of water or steam; in the case of organic solvents, the temperatures are above 30 ° C., preferably even above 50 ° C., even more preferably even above 60 ° C. and at most reach the boiling point of the respective organic liquid or the mixture of several organic liquids or one or more organic liquids Liquid (s) and water.
  • the pressure can be varied within a wide range and is usually, for example, 0.9 bar and above, preferably 1 to 1.12 bar, as far as steam distillation is concerned, and is, for example, 1 to 10 bar, preferably 1 to 5 bar, more preferably 1 to 4 bar, as far as solvent extraction is concerned.
  • the flow rate of the fluid medium (s) can be varied within a wide range and is dependent on a whole number of parameters, e.g. B. from the tank size, the size of the extraction container, the extraction time (which in turn depends heavily on the type of plant or parts of plants, their degree of comminution, etc.), the diameter of the supply line or the question of whether in countercurrent or parallel flow -Procedure is being worked on.
  • the fluid medium comprising at least one or more plant constituents is fed from the cylindrical container to at least one device for separating the plant constituent (s) from the at least one fluid medium and the separation into the at least one fluid medium and one or more plant ingredient (s) performed.
  • the fluid medium or fluids are derived from the cylindrical container and for distillation, decanting or other (e.g. chromatographic) separation of the plant ingredient (s) from the fluid medium / media supplied to respective separation devices.
  • a plurality of plant ingredients obtained by the route according to the invention can also be separated in one of the aforementioned ways, if this is necessary. In this way, highly pure plant constituents that are completely free of degradation products and / or secondary products and / or oxidation products can be obtained in high yield.
  • the covers or lower supply lines / discharge lines can easily be structurally varied by a person skilled in the art without thereby leaving the scope of the invention.
  • two fluid media are fed to the cylindrical container which contains the plants and / or plant parts in the second process step.
  • this can preferably be two liquids or two mixtures of liquids or two mixtures or solutions of one or more liquids and one or more gases or two mixtures or solutions of one or more liquids and one or more solids be, wherein two liquids that are not miscible with each other can also be present in a two-phase system.
  • two organic liquids such as an alcohol and an ether (e.g. ethanol and diethyl ether), water and an organic liquid such as an alcohol (e.g. Ethanol), an organic liquid (such as an ether, e.g. dipropyl ether) and a solution of e.g. B.
  • two fluid media are fed to the cylindrical container in two successive method steps.
  • the plant material or the plant parts can advantageously be treated with an organic solvent or a mixture of several organic solvents or with a mixture of at least one organic solvent and water in an earlier process step and treated extractively, and the plants or the Plant parts can be treated with water and / or steam in a subsequent process step - preferably in the same cylindrical container.
  • plants and / or parts of plants can be treated in an earlier method step with water or with a medium containing water, more preferably with steam containing water, and these are fed to the cylindrical container for the purposes of treatment during a subsequent process step, which is more preferably carried out in the same cylindrical container, the plants and / or plant parts are subjected to a treatment with one or more organic solvents), still more preferably a treatment with a mixture of several organic solvents or a mixture of water with one or more organic solvents ,
  • the step of supplying water or supplying a medium containing water, such as water vapor is a step of thermodynamic steam distillation.
  • Treatment of plants and / or parts of plants by means of thermodynamic steam distillation is described, for example, in German Patent No. 198 04 010, the disclosure of which is incorporated by reference into the present description.
  • a cylindrical container containing plants and / or plant parts such as, for example, a distillation container, is subjected to water vapor from below, i. H. from the container base.
  • the water vapor comes into contact with the plants or parts of plants, the water at least partially condenses on the plants or parts of plants, and the condensed (hot) water dissolves or suspends water-soluble plant constituents) to form an aqueous solution or suspension of the plant or plants - Ingredients ⁇ ) with water. Subsequent water vapor evaporates the solution or suspension formed and drives it to relatively colder plants or plant parts located further up in the cylindrical container, on which the steam condenses again.
  • the pressure can fluctuate over a relatively wide range.
  • pressure values in the range of the atmospheric spherical pressure preferred.
  • the process pressure is particularly advantageous at 1.013 ⁇ 0.1 bar.
  • the flow rate of the water vapor through the layering of plants or parts of plants can advantageously be in the range from 0.01 to 1 cm / s, preferably 0.1 to 0.3 cm / s.
  • the temperatures of the steam distillation are advantageously controlled so that they are in the range of the boiling point of the water under the pressure conditions of the process step.
  • the step of supplying one or more organic solvents to the cylindrical container is a step of flooding the cylindrical container with the organic solvent (s) while setting conditions for solvent extraction.
  • this takes place in such a way that the cylindrical container filled with plants and / or plant parts is filled with one or more organic solvents or a mixture of water and one or more organic solvents.
  • This (s) is / are at a temperature and / or is / are under a pressure which enables extraction of one or more plant constituent (s) from the plants and / or parts of plants into the solvent or the solvent mixture /enable.
  • continuous extraction conditions i.e.
  • a solvent or a solvent mixture or a mixture of one or more solvent (s) and one or more other components e.g. water and / or one or more acid (s) and / or one or more salt (s)
  • the solvent is continuously added to the base of the cylindrical container or withdrawing the solvent mixture with the plant ingredient (s) contained therein, which extract in the course of the contact of the organic solvent or the mixture containing one or more organic solvents with the plants and / or parts of plants from the latter was (n).
  • the flow rate of the solvent or the solvent-containing mixture through the cylindrical extraction container - depends on a large number of parameters (e.g. the tank size, the size of the extraction container, the extraction time (which in turn strongly depends on the type of plant or parts of the plant, its degree of comminution, etc.), the diameter the supply line or the question of whether the process is carried out in countercurrent or in parallel flow) and is preferably in a range which allows the extraction of the plant constituent (s) from the plants and / or parts of plants under the chosen reaction conditions , for example in the range from 0.01 to 1 cm / s, preferably in the range from 0.03 to 0.1 cm / s.
  • the temperature of the extraction process is dependent on the plant ingredients to be extracted), the plants (parts) used, the solvent (mixture) used and possibly also other parameters (e.g. degree of comminution of the plants (parts) or the like) and can be freely selected by a specialist taking into account the specifications of the aforementioned parameters.
  • Exemplary, non-limiting examples of the temperature are 0 to 130 ° C, preferably 40 to 70 ° C. It is also possible to use a temperature gradient over time in the course of the extraction process and thus possibly to take into account special requirements for the solvent extraction of one or more plant ingredients (s).
  • the pressure is also set as a function of one or more of the aforementioned parameters and can be chosen freely by a person skilled in the art, taking into account the specific circumstances.
  • a pressure gradient over the course of the extraction process can also be provided in order to take into account any special requirements for the solvent extraction of one or more plant ingredients (s).
  • a solvent extraction step carried out as a batch process can also be carried out.
  • the organic solvent (s) is / are fed to the cylindrical container in an amount sufficient to at least a large part of the loading filling the container with plants and / or parts of plants, preferably bringing the entire filling of the container with plants and / or parts of plants into contact with organic solvent or mixture containing organic solvent or to keep it in contact.
  • the solvent or the solvent-containing mixture remains in contact with the plants or parts of plants for a predetermined time, the extraction process taking place.
  • the time can be chosen freely depending on the aforementioned parameters, but in particularly preferred embodiments of the invention is in the range from 60 min to 24 h, more preferably in the range from 4 h to 8 h.
  • the selection of the further process parameters takes place within the scope of the ranges mentioned above; For example, temperatures in the range from 0 to 130 ° C., preferably in the range from 40 to 70 ° C., and pressures in the range from 0 to 5 bar, preferably in the range from 0 to 2.5 bar, are selected for a “static” solvent extraction ,
  • the solvent extraction step is a process step consisting of two separate extraction steps. This may be possible, for example, if one plant material (plants and / or plant parts) contains several plant ingredients which can be extracted under conditions of solvent extraction, one of which can be extracted from the plant material with a solvent or a solvent mixture or under conditions, while the other (or the others) is / are not extractable with this solvent or with this solvent mixture or under these extraction conditions, but only with another solvent or with a different or differently composed (for example more polar or less polar) mixture and / or under different extraction conditions.
  • the solvent extraction step is repeated, optionally also repeated twice or more so different plant ingredients or to obtain different fractions of plant ingredients from the plants or parts of plants.
  • the solvent extraction process step can also be a generally customary extraction step using one or more solvents known from the prior art.
  • the cover and, if appropriate, corresponding supply or discharge lines
  • the second process step before supplying a fluid medium (if necessary with the necessary supplies). or drains) on the container head (and possibly also another closure at the lower end of the container) in a manner which closes / reseals the cylindrical container as a whole.
  • the different covers (and, if applicable, lower closures) applied in the first process step and in the second process step are adapted to the tasks in the respective step, and in particular they have the necessary supply lines and discharge lines for the (possibly containing one or more plant ingredient (s) ) fluid media and closure elements with which the respective cover on the container head (and possibly also on the lower end of the container) can be fixed in such a way that a suitable, if necessary, closed system is created for steam distillation on the one hand and solvent extraction on the other.
  • a uniform container head and a uniform container foot can be used for all process variants, and only the respective supply lines conditions and derivatives on the tank head and tank base of the respective process task - steam distillation or solvent extraction - adapted.
  • the treatment of the plants and / or plant parts in the cylindrical vessel takes place in such a way that a fluid medium containing water vapor is supplied to the cylindrical container in an earlier process step, conditions of steam distillation are set, draws the mixture of water-containing fluid medium and plant ingredient (s) at the upper end of the cylindrical container through a water vapor distillation cover of the container into a condenser for condensation, the water vapor distillation cover of the container against a solvent extraction cover of the container and if necessary, the lower steam supply of the container is replaced by a lower container closure for withdrawing the mixture of solvent (s) and plant ingredient (s) and, in a subsequent process step, the cylindrical container via the L solvent extraction cover supplies a fluid medium containing one or more organic solvents, sets conditions for solvent extraction, and the mixture of one or more organic solvents containing fluid medium and plant ingredient (s) at the foot of the cylindrical container withdraws.
  • the solutions or suspensions or extracts obtained in the preceding process steps are treated in such a way that the plant ingredients obtained from the plants or parts of plants are separated from the fluid medium / media.
  • This can be done in any way known to those skilled in the art. Examples are separation by decanting or separation or by layering due to different densities in a suitable vessel (e.g. a settling vessel or a separating funnel), separation by distillation, elution, filtration, sedimentation, centrifugation, pervaporation, rectification, separation by Adsorption on a suitable adsorbent, separation by chromatographic methods, etc., to name just a few.
  • a suitable vessel e.g. a settling vessel or a separating funnel
  • separation by distillation, elution, filtration, sedimentation, centrifugation, pervaporation, rectification separation by Adsorption on a suitable adsorbent, separation by chromatographic methods, etc., to name just a few.
  • the plant ingredient (s) extracted from the plants or parts of plants are obtained in pure form, and the products are essentially free of by-products, decomposition products or degradation products.
  • the pure form obtained they are far superior to plant ingredients obtained by previous methods and can be used directly as fragrances, for example for the cosmetics industry, flavorings, for example for the food industry, etc.
  • the entire process or also individual steps of the process can be carried out under a protective gas.
  • a protective gas such as nitrogen (N), argon (Ar) or a mixture of protective gases can be used.
  • the device used for the method is provided with corresponding supply lines and discharge lines for the protective gas (s).
  • the process according to the invention is carried out with particular advantage in such a way that a cylindrical container which is closed except for inlets and outlets is filled with a previously measured amount of plants and / or plant parts in such a density that fluid contact of the plants and / or parts of plants with at least one fluid medium is possible; - Steam and / or a mixture of water vapor and water as a fluid medium are fed to the cylindrical container in a first process step under conditions in which a thermodynamic steam distillation of one or more water-soluble or water-suspendable plants Ingredient (s) between the plants and / or plant parts on the one hand and the fluid medium water / water vapor on the other hand is possible; Water as the fluid medium charged with one or more plant constituent (s) from the cylindrical container supplies at least one device for separating the plant constituent (s) from water / water vapor as the at least one fluid medium and separately the separation into Water as the at least one fluid medium and one or more plant ingredient (s); the cover of the closed cylindrical container for the Wasserdampfde- • stillation
  • the inventive device (1) for obtaining one or more plant ingredients ⁇ ) from plants and / or parts of plants by treating the plants and / or parts of plants with at least one fluid medium under conditions of pressure and temperature at which the plants and / or Plant parts at least partially deliver one or more plant constituent (s) to the at least one fluid medium, and separating the plant constituent (s) from the at least one fluid medium comprises a preferably cylindrical container 11 for holding plants and / or parts of plants and their treatment.
  • the cylindrical container 11 can be a conventional container made of a material from the group glass, for example with glass, plastics) or the like.
  • the cylindrical container 11 may optionally have a shape other than the cylindrical shape or may have a shape that is partially cylindrical and partially deviates from the cylindrical shape.
  • a cylindrical container 11 is preferably used, and the invention is described below with reference to the exemplary cylindrical container 11, without being limited thereto.
  • the cylindrical container 11 is insulated against heat loss.
  • Thermal insulation can be conventional thermal insulation, comprising, for example, a slightly heat-conducting or non-heat-conducting material as a covering around the container 11 over a part or the like full axial length, possibly in turn surrounded by an outer covering holding the heat-conducting material, which can consist, for example, of a plastic material or a metal sheet.
  • casings insulating against heat loss are known per se from the prior art; those skilled in the art can choose the materials suitable for the present invention from the available materials.
  • the cylindrical container 11 has a container head 111 at its upper end (in the usual configuration) and a container base 112 at its lower end, which is arranged away from the upper end. By means of devices to be described in detail below on the container base 112 and on the container head 111, the container 11 is essentially closed (viewed from supply lines and discharge lines at the upper and / or lower end).
  • the cylindrical container 11 serves to hold the plants or plant parts to be treated and to treat them with at least one fluid medium.
  • an attachment 17 which, among other things, serves to close the container 11 downwards.
  • the attachment 17 is removably arranged on the container base 112 and has an opening 18 for feeding in a fluid medium for steam distillation, for example for feeding in water vapor, and / or an opening 19 for withdrawing a mixture of plant constituent (s) / fluid medium for the Solvent extraction.
  • the attachment 17 for the container base comprises a sieve base 171 with a plurality of openings of more or less the same size distributed over its area, which allow passage of fluid media and / or plant constituents, but not of plants or parts of plants.
  • the sieve bottom 171 thus serves on the one hand as a device on which the bed of plants or parts of plants rests after it was filled into the cylindrical container, and on the other hand serves as a device which ensures a uniform distribution of the flow of the fluid medium when the flow of the bed of plants or plant parts flows from below and thus prevents the formation of flow channels of the fluid medium in the plant bed.
  • the container head 111 is provided according to the invention with a steam distillation cover 12 with attachable devices 22 for condensing the mixture of water-containing fluid medium / plant ingredient (s) and devices 23 for collecting the condensate and separating the condensate components and devices 122 for fluid tight connection to the container head 111 and a solvent extraction cover 13 to be used as an alternative to the steam distillation cover 12 with connectable devices 131 for supplying fluid medium for the solvent extraction and devices 132 for fluid-tight connection to the container head 111.
  • the covers 12, 13 also each have a device with which it is possible to alternately bring the covers into contact with the container head 111 and on it in the closed position.
  • Devices of this type can be joints which are attached to the container head 111 on the one hand and to a cover 12, 13 on the other hand.
  • the two joints are arranged opposite one another on the circumference of the container head 111, so that in the embodiment of the invention thus constructed, the covers 12, 13 can be brought into position in such a way that the one cover 12 around the joint belonging to it is folded away from the container head 111, after which the other cover 13 is opened around the joint belonging to it onto the container head 111.
  • the devices consist of axes mounted parallel to the axis of the cylindrical container 11, about which the two covers 12, 13 are pivotally mounted and can be pivoted alternately onto the container head 111.
  • the cover 12 is released and about one axis pivoted away from the container head 111, after which the other cover 13 is pivoted about the other axis on the container head 111 and fixed thereon.
  • the other method step can begin.
  • the device according to the invention can also have a single, optionally fixed, but removable cover on the container head 111 and / or a single, if appropriate, have a fixed but removable attachment on the container base 112.
  • the supply lines and discharge lines required for the respective method steps can alternatively be attached to such a fixed cover and / or such a fixed attachment or removed by pivoting them away.
  • This alternative embodiment facilitates and accelerates the "reconstruction” of the plant and enables a rapid change from the "steam distillation” alternative to the "solvent extraction” alternative and vice versa. This embodiment is shown in FIGS. 3A and 3B.
  • the device can comprise further devices which are connected to the cylindrical container 11 or with the attachment 17 at the foot of the cylindrical container 11 or one of the covers 12, 13 of the cylindrical see container 11 are connected and thus form a system according to the functional diagram shown in Figure 1 with one or two separate circuits, ie a water vapor distillation circuit, a solvent extraction circuit or a combination of a water vapor distillation circuit and a solvent extraction circuit.
  • the steam distillation cycle is preferably run first, followed by a solvent extraction cycle.
  • the device comprises a steam generation unit 14. This is part of the water vapor distillation circuit and feeds water vapor or a mixture of water and water vapor via a line 141 into the attachment 17 on the container base 112 of the cylindrical container 11, so that the steam stratifies the plants or plant parts from the lower end of the container 11 can flow to.
  • the device can comprise a heat exchanger together with the other devices or in their place. This is used to preheat the solvent used in a possible solvent extraction step.
  • Another possible device 1 can be a storage unit 16 for an organic solvent or a mixture comprising at least one organic solvent.
  • the latter units are connected to one another and / or to the cylindrical container 11 via suitable lines 131, 161.
  • the line connection can be a flow connection (for example steam generation unit ⁇ attachment 17 to the container base 112 or heat exchanger ⁇ solvent storage unit 16) or a functional connection (steam generation unit 14 ⁇ heating side of the heat exchanger).
  • devices 121 can be connected to the water vapor distillation cover 12 in preferred embodiments of the invention, which serve to discharge the product, separate it from the fluid medium and obtain the pure product.
  • a discharge line (spirit pipe) 21 for the steam or the condensate from the fluid medium of steam distillation e.g.
  • the solvent extraction cover 13 which can alternatively be attached to the container head 111, comprises further connectable devices such as, for example, one (or, in the case of several solvents, several) with the storage unit 16 (or in the case of more solvents, if necessary, with a plurality of storage units 16) in fluid connection with the solvent supply lines ) 131, and one (in the case of several solvents, possibly also several) heat exchangers for setting the optimum solvent temperature; in the case of several solvents, a device for mixing the different solvents can also be provided (not shown).
  • the further embodiment of the invention is preferred, according to which the steam distillation cover 12 for the container head 111 and the solvent extraction cover 13 for the container head 111 can be movably attached to the container head 111 and, alternatively, can be attached to the container head 111 in a fluid-tight manner.
  • the moveable attachment can be a hinge for folding the two covers 12, 13 or a pivoting device for pivoting the two covers from a non-functional side position to a fluid-tight position on the container head 111 in function for steam distillation (Cover 12) or for solvent extraction (cover 13).
  • the fluid-tight seal between one of the covers 12, 13 and the container head 111 can be done in any way, as long as the goal of a fluid-tight closure of the cylindrical container is achieved.
  • One (or more) seal (s) is preferably used for this purpose.
  • the most important advantage of the device according to the invention over devices for obtaining plant constituents from the prior art, for example over a device according to German Patent No. 198 04 010, is the possibility of double use of the cylindrical container for both an aqueous and distillative Treatment of plants or parts of plants to obtain water-soluble or water-soluble plant ingredients as well as treatment of plants or parts of plants with at least one solvent to obtain non-water-soluble or only suspendable plants Ingredients.
  • plants or parts of plants which contain both one or more steam-volatile plant ingredient (s) and one or more organic phase-soluble or extractable ( n) contain plant ingredient (s) of economic interest, preferably first subjected to a steam distillation step in the steam distillation circuit of the device according to the invention.
  • the steam-volatile plant ingredients are obtained in pure form.
  • the steam supply in the steam generating unit 14 is interrupted, the device 121 consisting of the spirit tube 21, the cooler 22 and the template 23 is separated from the upper cover 12 of the cylindrical container, and the upper cover 12 is folded away or pivoted away from the container head 111.
  • the cover 13 is folded or swiveled onto the container head 111 and closed there in a fluid-tight manner, and the circuit for the supply of organic solvent or a solvent mixture comprising at least one organic solvent is (also by attaching the lower attachment 17 for the solvent supply ) closed, after which the solvent extraction can begin.
  • the advantage of this process is that the readily (water vapor) volatile plant ingredients in a first, thermodynamically controlled process step that runs under mild conditions or, if necessary, also takes place under certain overpressure or underpressure ratios in the purest form and good yield can be won. These components are not subject to temperature or oxygen pollution, so that oxidation or decomposition or degradation reactions are largely avoided, which benefits the quality of the products obtained.
  • the further processing of the plant material, which has already been "extracted” in the first step, can then take place in the same cylindrical vessel, which not only makes the (earlier) transfer of the hot plant material superfluous, but also prevents the entry of oxygen to this hot material (at Decanting or degradation reactions of other plant constituents still present in the plant material. Furthermore, the thermal energy of the plant material can be used for the second extraction step (which often takes place at elevated temperature). Previously common extraction plants left a two-stage process, especially under Preceding a steam distillation, not too.
  • the present invention permits double use even in existing systems which are converted accordingly or provided with the system according to the invention of alternatively usable covers 12, 13 or lower attachments 17.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • General Preparation And Processing Of Foods (AREA)

Abstract

L'invention concerne un procédé permettant d'extraire des substances de végétaux et/ou de fragments de végétaux. L'invention concerne également un dispositif d'extraction de substances de végétaux et l'utilisation du dispositif dans le procédé susmentionné.
PCT/EP2003/004150 2002-04-18 2003-04-22 Procede et dispositif permettant d'extraire des substances de vegetaux WO2003086566A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003233038A AU2003233038A1 (en) 2002-04-18 2003-04-22 Method and device for obtaining plant ingredients

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10217353.2 2002-04-18
DE10217353A DE10217353A1 (de) 2002-04-18 2002-04-18 Verfahren und Vorrichtung zur Gewinnung von Pflanzen-Inhaltsstoffen

Publications (2)

Publication Number Publication Date
WO2003086566A2 true WO2003086566A2 (fr) 2003-10-23
WO2003086566A3 WO2003086566A3 (fr) 2004-02-19

Family

ID=29224558

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2003/004150 WO2003086566A2 (fr) 2002-04-18 2003-04-22 Procede et dispositif permettant d'extraire des substances de vegetaux

Country Status (3)

Country Link
AU (1) AU2003233038A1 (fr)
DE (1) DE10217353A1 (fr)
WO (1) WO2003086566A2 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008148281A1 (fr) * 2007-06-08 2008-12-11 Shenzhen Zofu Technology Co., Ltd. Procédé et dispositif permettant de préparer une solution avec un équipement pour préparer du thé parfumé
WO2009122337A1 (fr) * 2008-04-04 2009-10-08 Consorzio Powerfeed Pavia Procédé d'extraction de composants actifs à partir de lippia polystachya et extrait ainsi obtenu
CN112842899A (zh) * 2021-02-03 2021-05-28 陕西中医药大学 一种用于中药提取、精制、收膏及减压干燥的一体装置
WO2022079171A1 (fr) * 2020-10-16 2022-04-21 L'oreal Concrete et absolue de parfum obtenues par extraction de solvant heterocyclique a partir de matieres naturelles solides
FR3134821A1 (fr) * 2022-04-20 2023-10-27 L'oreal Concrete et absolue de parfum obtenues par extraction de solvant ether a partir de matieres naturelles solides

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012006145B4 (de) * 2011-05-13 2013-07-25 Helmut Rausche Verfahren zur Gewinnung von Aromen aus Biomaterial

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5026549A (en) * 1988-08-26 1991-06-25 Biolandes Technologies Method of extracting solid materials using a solvent and an apparatus for implementing same
EP0434851A1 (fr) * 1988-09-19 1991-07-03 Tigney Technology Inc. Procédé d'obtention de fibres cellulosiques intactes et séparées et produits ainsi obtenus
US5441612A (en) * 1994-06-30 1995-08-15 Florasynth, Inc. Radiation-enhanced recovery of maltol
US5525746A (en) * 1992-12-31 1996-06-11 Univesity Research & Marketing Inc. Method for selective extraction of compounds from carbonaceous materials
EP0812903A1 (fr) * 1994-04-05 1997-12-17 Agritech International, L.L.C. Extraction d'huile à partir de parties de plantes oléagineuses
DE19804010A1 (de) * 1998-02-02 1999-08-12 Bayerische Landesanstalt Fuer Verfahren und Vorrichtung zur Gewinnung von Pflanzen-Inhaltsstoffen
US6111119A (en) * 1999-01-14 2000-08-29 Cocotech, Inc. Process for removing oil from food products
US6344575B1 (en) * 1999-02-10 2002-02-05 Phytopharm Pic Extraction of volatile oils

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5026549A (en) * 1988-08-26 1991-06-25 Biolandes Technologies Method of extracting solid materials using a solvent and an apparatus for implementing same
EP0434851A1 (fr) * 1988-09-19 1991-07-03 Tigney Technology Inc. Procédé d'obtention de fibres cellulosiques intactes et séparées et produits ainsi obtenus
US5525746A (en) * 1992-12-31 1996-06-11 Univesity Research & Marketing Inc. Method for selective extraction of compounds from carbonaceous materials
EP0812903A1 (fr) * 1994-04-05 1997-12-17 Agritech International, L.L.C. Extraction d'huile à partir de parties de plantes oléagineuses
US5441612A (en) * 1994-06-30 1995-08-15 Florasynth, Inc. Radiation-enhanced recovery of maltol
DE19804010A1 (de) * 1998-02-02 1999-08-12 Bayerische Landesanstalt Fuer Verfahren und Vorrichtung zur Gewinnung von Pflanzen-Inhaltsstoffen
US6111119A (en) * 1999-01-14 2000-08-29 Cocotech, Inc. Process for removing oil from food products
US6344575B1 (en) * 1999-02-10 2002-02-05 Phytopharm Pic Extraction of volatile oils

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008148281A1 (fr) * 2007-06-08 2008-12-11 Shenzhen Zofu Technology Co., Ltd. Procédé et dispositif permettant de préparer une solution avec un équipement pour préparer du thé parfumé
WO2009122337A1 (fr) * 2008-04-04 2009-10-08 Consorzio Powerfeed Pavia Procédé d'extraction de composants actifs à partir de lippia polystachya et extrait ainsi obtenu
WO2022079171A1 (fr) * 2020-10-16 2022-04-21 L'oreal Concrete et absolue de parfum obtenues par extraction de solvant heterocyclique a partir de matieres naturelles solides
FR3115292A1 (fr) * 2020-10-16 2022-04-22 L'oreal Concrete et absolue de parfum obtenues par extraction de solvant heterocyclique a partir de matieres naturelles solides
CN112842899A (zh) * 2021-02-03 2021-05-28 陕西中医药大学 一种用于中药提取、精制、收膏及减压干燥的一体装置
FR3134821A1 (fr) * 2022-04-20 2023-10-27 L'oreal Concrete et absolue de parfum obtenues par extraction de solvant ether a partir de matieres naturelles solides

Also Published As

Publication number Publication date
DE10217353A1 (de) 2003-11-13
WO2003086566A3 (fr) 2004-02-19
AU2003233038A8 (en) 2003-10-27
AU2003233038A1 (en) 2003-10-27

Similar Documents

Publication Publication Date Title
EP0081231B1 (fr) Procédé pour la production des substances aromatiques à partir d'un extrait de tabac
DE2818852C2 (de) Verfahren zur Herstellung eines Extraktes und Vorrichtungen zur Durchführung des Verfahrens
DE1493190C3 (de) Verfahren zur Trennung von Stoffgemischen
DE3424614C2 (fr)
DE3033729A1 (de) Verfahren und vorrichtung zum abscheiden geloester organischer fluessiger substanzen von ihren loesungsmittelgemischen
DE1598017A1 (de) Vorrichtung und Verfahren zum Auffangen von gaschromatographischen Fraktionen
DE3148335C2 (de) Verfahren zur Gewinnung von Aromastoffen aus Tabak und deren Verwendung
EP3092054B1 (fr) Traitement de séparation d'un mélange gazeux constitué d'un flux de produit d'un réacteur à diméthyléther
EP2644039A1 (fr) Procédé d'obtention d'arômes à partir de matérial biologique
DE4002161C2 (fr)
EP0553658A2 (fr) Compositions pharmaceutiquement actives à de Tanacetum parthenium, procédé d'extraction et médicament
WO2003086566A2 (fr) Procede et dispositif permettant d'extraire des substances de vegetaux
EP3092053B1 (fr) Procédé de séparation d'un flux de produit d'un réacteur à diméthyléther
EP3652138B1 (fr) Procédé et installation de fabrication de propylène par combinaison de déshydrogénation de propane et procédé de vapocraquage avec stages de pre-séparation dans les deux procédés pour éliminer hydrogène et méthane
DE69723294T2 (de) Materialien behandlung
DE102015119154A1 (de) Verfahren und Vorrichtung zum Herstellen eines Aromastoffkonzentrats aus einem alkoholhaltigen Lebensmittel
DE2327106A1 (de) Verfahren und vorrichtung zum trennen einzelner komponenten aus einem stroemungsgemisch
DE19800330C2 (de) Pharmazeutisch wirksamer CO¶2¶-Extrakt aus Tanacetum parthenium
WO1994026683A1 (fr) Procede et dispositif permettant de produire un squalene a partir de residus d'huile d'olive
DE3038870A1 (de) Verfahren zur dampfgewinnung
DE3725228A1 (de) Verfahren zur gewinnung von reinen aromaten
DE60030299T2 (de) Vorrichtung und verfahren zur verminderung von restlösungsmittelgehalten
DE102012006145A1 (de) Verfahren zur Gewinnung von Aromen aus Biomaterial
DE3544855A1 (de) Verfahren zur abtrennung von c(pfeil abwaerts)5(pfeil abwaerts)(pfeil abwaerts)+(pfeil abwaerts)-kohlenwasserstoffen aus einem gasstrom
DE102019115388A1 (de) Verfahren und Anlage zur Gewinnung eines Olefins

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A2

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NO NZ OM PH PL PT RO RU SD SE SG SK SL TJ TM TN TR TT TZ UA UG US UZ VN YU ZA ZM ZW

AL Designated countries for regional patents

Kind code of ref document: A2

Designated state(s): GH GM KE LS MW MZ SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LU MC NL PT RO SE SI SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
REG Reference to national code

Ref country code: DE

Ref legal event code: 8642

122 Ep: pct application non-entry in european phase
NENP Non-entry into the national phase

Ref country code: JP

WWW Wipo information: withdrawn in national office

Country of ref document: JP